5-Membered rings – 2N 305
7-amino-4,6-dinitrobenzofuroxan (77) (ADNBF) is more impact insensitive than 4,6-
dinitrobenzofuroxan. ADNBF (77) has been prepared^48 from the nitration ofm-nitroaniline
(75), followed by reaction of the product, 2,3,4,6-tetranitroaniline (76), with sodium azide in
acetic acid; the latter reagent resulting in displacement of the labilem-nitro group of (76)
and spontaneousin situcyclization of the resultingo-nitroarylazide. ADNBF has also been
synthesized from the nitration of 6-chlorobenzofuroxan, followed by reaction with ammo-
nia in methylene chloride.^48 A more unusual route to ADNBF involves the reaction of 4,6-
dinitrobenzofuroxan (DNBF) with a source ofN-formyl anion and oxidation of the resulting
Meisenheimer complex with nitric acid.^49 ADNBF has excellent overall properties (calculated
VOD∼7900 m/s,d= 1 .90 g/cm^3 and m.p. 270◦C) and is under advanced development in
the US.
Cl
NO 2
Cl
78
Cl
79
O 2 N
Cl N 3
O 2 N NO 2
Cl
Cl
80
N 3
NO 2
NO 2
O 2 N
Cl
N
O
NO 2
Cl
81
O 2 N
N Cl
O
NO 2
NH 2
H 2 N
N O 2 N
O
N
NO 2
N
O O
N
O
N
O
HR
O K
+
83, R = NHOH
82
(DADNBF)
NaN 3 , DMF 100 % HNO 3
PhCH 3
heat
PhCH 3 , NH 3
- NH 2 OH.HCl,
KOH (aq) - H+
Figure 7.31
5,7-Diamino-4,6-dinitrobenzofuroxan (DADNBF) (82), an impact insensitive high perfor-
mance explosive (VOD∼8050 m/s,d= 1 .91 g/cm^3 ), has been prepared in four steps from
1,3,5-trichloro-2,4-dinitrobenzene (78),^50 and also by treating the Meisenheimer complex
(83)^51 with excess hydroxylamine hydrochloride in aqueous base. DADNBF has also been
synthesized in five steps starting from 2-nitroaniline.^51
2 N NH 2 O 2 NH NO 2
Cl
Cl
NO 2
85
H
N
H
N
NO 2
NO 2
NO 2
O 2 N
O 2 N
Cl O 2 N Cl
H
N
H
N
Cl Cl
H
N
H
N
NO 2
NO 2
NO 2
NO 2
NO 2
NO 2
NO 2
NO 2
O 2 N NO 2
O 2 N
O 2 N
O 2 N
O 2 N
O 2 N
O 2 N
N
O
N N
O
N
NaHCO 3
+
86
87
- NaN 3
- heat, -N 2
88
84
100 % HNO 3 ,
H 2 SO 4
2
OO
Figure 7.32